CN109799204B - Low concentration COD measuring device based on spectrum method - Google Patents
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Abstract
The invention provides a low-concentration COD measuring device based on a spectrum method, which comprises a light source, a collimation system, a sample pool, a convergence system and an optical signal detection system, wherein the inner wall of the sample pool is provided with a first optical reflection end surface and a second optical reflection end surface which are opposite, a first quartz optical window and a first plane reflector are sequentially arranged on the first optical reflection end surface, and the first quartz optical window is a light source incidence surface; a second plane reflector and a second quartz optical window are sequentially arranged on the second optical reflection end face, and the second quartz optical window is an emergent face of the light source; light emitted by the light source is changed into parallel light through the collimation system, the parallel light enters the sample cell through the incident surface of the sample cell, the parallel light is emitted from the emergent surface of the sample cell after being reflected for multiple times by the first plane reflector and the second plane reflector and absorbed by liquid to be detected, and the parallel light enters the optical signal detection system after passing through the convergence system; compared with the traditional device using a straight line measuring light path, the invention greatly reduces the detection limit of COD concentration.
Description
Technical Field
The invention relates to the field of water quality detection and analysis, in particular to the technical field of a COD detection method and environmental optical detection, and specifically relates to a low-concentration COD measuring device based on a spectrum method.
Background
Chemical Oxygen Demand (COD) refers to the amount of oxidant consumed when reducing substances in a water body are oxidized by a strong oxidant under a certain condition, and is a comprehensive index for representing the reducing substances in the water, wherein the amount of oxidant is converted into the concentration of oxygen in mg/L. In recent years, the national economy of China is rapidly developed, but the environmental pollution problem is increasingly serious. Especially the problem of water pollution. COD can be used for judging the relative content of organic matters in a water body, and is one of the most important organic pollution comprehensive indexes in environmental monitoring. The method for measuring the COD of the water body mainly adopts an alkaline potassium permanganate colorimetric method at present, and is also a method commonly adopted in a laboratory at present, the method is accurate in measurement and good in reproducibility, but the steps of water sample sampling and transportation, complex reagent reaction pretreatment, measurement and analysis and the like are required in the test process, the operation is complex, the analysis time is long, a chemical reagent is required to be added, the added chemical substances easily cause secondary pollution to the environment, the reagent amount is large, the mass rapid measurement is difficult, and the requirement of on-site/on-line environment monitoring cannot be met.
The method for measuring COD by adopting the ultraviolet absorption spectrometry has the advantages that no chemical reagent is required to be added, direct measurement can be realized without pretreating a water sample, the detection speed is high, complicated operation steps and secondary pollution to the environment are avoided, and the method is suitable for on-site/on-line monitoring.
At present, the detection limit of COD measurement by an ultraviolet absorption spectrometry is generally more than 10mg/L, the COD content in drinking water and seawater is lower, generally 3mg/L, and is lower than the detection limit of COD measurement by the ultraviolet absorption spectrometry, so the COD in the water environment can only adopt an alkaline potassium permanganate colorimetric method, and the on-site/on-line monitoring and control of COD in seawater, drinking water and the like in China are restricted.
At present, the market urgently needs a detection device which has high detection speed, can avoid secondary pollution and is suitable for low-concentration COD.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a low-concentration COD measuring device based on a spectrum method, wherein a sample cell increases the reflection times of incident light, changes the measuring optical path and accordingly enlarges the measuring range of COD concentration.
According to the purpose of the invention, the low-concentration COD measuring device based on the spectrum method comprises a light source, a collimation system, a sample cell, a convergence system and an optical signal detection system, wherein the inner wall of the sample cell is provided with a first optical reflection end face and a second optical reflection end face which are opposite, a first quartz optical window and a first plane reflector are sequentially arranged on the first optical reflection end face, and the first quartz optical window is an incident face of the light source; a second plane reflector and a second quartz optical window are sequentially arranged on the second optical reflection end face, and the second quartz optical window is an emergent face of the light source;
the light emitted by the light source is changed into parallel light through the collimation system, the parallel light enters the sample cell through the first quartz light window of the sample cell, the parallel light is emitted from the second quartz light window of the sample cell after being reflected for multiple times by the first plane reflector and the second plane reflector and absorbed by liquid to be detected, and then enters the optical signal detection system after passing through the convergence system;
the optical signal detection system is used for splitting and detecting incident light, acquiring light intensity signals of various wavelengths, and calculating the light intensity signals to obtain the COD concentration of the detected liquid.
The device adopts an ultraviolet spectrophotometry method, and can realize the direct measurement of the COD concentration in the water body. The sample cell makes the measuring optical path lengthen, enlarges the measuring range of COD concentration and can measure the COD with lower concentration. The method has the advantages of high detection speed, no complicated experimental steps, no need of adding chemical reagents, and no secondary pollution to water.
Preferably, an included angle θ is set between the first planar reflector and the second planar reflector, and the measurement optical path is changed by setting the included angle θ between the first planar reflector and the second planar reflector, so as to change the COD concentration measurement range.
When the sample cell is manufactured, the included angle theta between the first plane reflector and the second plane reflector is set through an angle measuring device to change the measuring optical path, and different theta correspond to different measuring optical paths, so that the measuring range of the COD concentration is changed. Due to the angle theta of the plane mirror, the light is reflected multiple times in the sample cell. Compared with the traditional linear measuring light path, the measuring light path is increased, so that the detection limit of COD concentration is greatly reduced, the detection sensitivity is improved, and the low-concentration detection of COD can be realized.
The reflection times of light in the sample cell determine the measurement optical path, the more the reflection times are, the larger the measurement optical path is, the lower the detection limit of COD concentration is, the larger the measurement range is, the reflection times can be changed by setting the difference of the included angle theta of the two plane mirrors, so that the optical path is changed, and the measurement range of the COD concentration is enlarged. For example, the angle θ may preferably be between 0 and 2 °.
In the invention, the sample pool is used for containing the water sample to be detected. The sample cell adopts a closed sample cell or an open sample cell. For example, the closed sample cell is a closed strip hexahedron, and comprises a bottom plate and an upper cover plate, wherein a water inlet and a water outlet are formed at the front end and the rear end of the sample cell; the left and right surfaces are a first optical reflection end surface and a second optical reflection end surface; the bottom plate and the upper cover plate are made of black light-tight materials. The sample pool can also adopt an open type sample pool, the open type sample pool is provided with a rectangular channel, the rectangular channel is used for the inflow of the tested water sample, and the open type sample pool is suitable for being thrown into a water body for online measurement. The open type sample cell is not provided with a bottom plate, an upper cover, a front end face and a rear end face, only comprises a left end face and a right end face, a rectangular channel into which a measured water sample can flow is formed, and the left end face and the right end face are respectively a first optical reflection end face and a second optical reflection end face.
Preferably, the first plane reflector and the second plane reflector are made of quartz glass materials, and the rear surfaces of the first plane reflector and the second plane reflector are plated with ultraviolet enhanced reflecting films for enhancing the reflection of ultraviolet band light. The ultraviolet reflection film can also be formed by superposing a piece of quartz glass and an ultraviolet enhancement reflector, so that the damage of a water body to the ultraviolet reflection film can be avoided. Thus, the ultraviolet enhanced reflection films are respectively plated on the rear surfaces, and the damage of the water body to the ultraviolet enhanced reflection films can be avoided.
Preferably, the first quartz optical window, the second quartz optical window and the converging system are selected as quartz lenses to reduce absorption of light in the ultraviolet band and improve the transmittance of ultraviolet light.
Preferably, the parallel light is perpendicularly incident to the first quartz light window incident surface of the sample cell, so as to reduce the dispersion of the incident light with different wavelengths due to different refractive indexes of the liquid.
Preferably, the light source is any one of a xenon lamp broadband light source, a pulsed xenon lamp broadband light source, a deuterium lamp broadband light source, a narrow-band LED or a laser narrow-band light source.
Preferably, the function of the collimation system is to obtain parallel light, and the collimation system adopts a concave reflector or a quartz collimator; the concave reflector is plated with an ultraviolet enhanced reflecting film; for flexibility of the optical path, light can be coupled to the optical fiber through a converging mirror, and the light is changed into parallel light through a collimating mirror at the output end of the optical fiber. Preferably, the function of the converging system is to converge parallel light into the detection system, and the converging system adopts a concave reflecting mirror or a quartz converging mirror; the concave reflector is plated with an ultraviolet enhanced reflecting film; for flexibility of the optical path, it is also possible to couple parallel light to the optical fiber by means of a converging mirror, and to converge the light at the output end of the optical fiber by means of the converging mirror.
Preferably, the detection system is used for performing light splitting detection on an optical signal, and the optical signal detection system adopts a spectrometer or an optical filter and a detector; further, the detector is any one of a linear array CCD, an area array CCD, a photodiode array, a photomultiplier tube or a photocell. In addition, in the actual test process, the sample cell can be placed on an angle rotating platform, the rotating angle of the sample cell can be controlled, the angle of the light beam incident on the sample cell can be slightly adjusted (the angle ranges from 0 to 5 degrees), and the reflection times can be rapidly changed to change the measuring optical path.
The light source, the collimation system, the convergence system and the specific devices and structures in the optical signal detection system in the device are respectively selected according to application requirements. If any optical lens needing light reflection, light condensation and the like, such as a concave reflector or a plane reflector, is involved in the device, the surface of the lens needs to be plated with an ultraviolet enhanced reflection film to enhance the reflection efficiency of ultraviolet band light, and all involved lenses are quartz lenses to improve the ultraviolet transmittance.
Compared with the prior art, the invention has the following beneficial effects:
the invention sets the sample cell with the plane reflecting mirror on the two inner walls, and can make light reflect in the sample cell for multiple times by adjusting the angle of the light beam incident to the sample cell or setting different included angles of the plane reflecting mirror of the sample cell.
The invention can realize direct measurement of COD concentration in the water body, has high detection speed by adopting an ultraviolet spectrophotometry method, avoids fussy experimental steps, does not need to introduce chemical reagents, and avoids secondary pollution to the water body.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a schematic diagram of the optical path structure in a preferred embodiment of the present invention;
FIG. 2 is a preferred embodiment of the present invention in which the alignment system is connected by optical fibers;
FIG. 3 is a convergence system connected by optical fibers in a preferred embodiment of the invention;
FIG. 4 is a closed sample cell in a preferred embodiment of the invention;
FIG. 5 is an open sample cell in a preferred embodiment of the invention;
FIG. 6 shows the test results of a preferred embodiment of the apparatus of the present invention;
the scores in the figure are indicated as: the device comprises a light source 1, a collimation system 2, a sample cell 3, a convergence system 4, an optical signal detection system 5, an optical fiber 6, a first plane reflector 7, a second plane reflector 8, a first quartz optical window 9, a second quartz optical window 10, a water inlet 11 and a water outlet 12.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
As shown in fig. 1-6, a schematic structural diagram of a preferred embodiment of an apparatus for measuring low concentration COD based on spectroscopy is shown, and the schematic structural diagram includes a light source 1, a collimating system 2, a sample cell 3, a converging system 4 and a signal detecting system 5, wherein an inner wall of the sample cell 3 is provided with a first optical reflection end face and a second optical reflection end face which are opposite to each other, a first quartz optical window 9 and a first plane mirror 7 are sequentially arranged on the first optical reflection end face, and the first quartz optical window 9 is an incident face of the light source 1; a second plane reflector 8 and a second quartz optical window 10 are sequentially arranged on the second optical reflection end face, and the second quartz optical window 10 is an emergent face of the light source 1;
as shown in fig. 1-2, light emitted from the light source 1 is converted into parallel light by the collimating system 2, as shown in fig. 4, the parallel light enters the sample cell 3 from an incident surface of the sample cell 3, i.e., the first quartz optical window 9, and after being reflected for multiple times by the first planar reflector 7 and the second planar reflector 8 and absorbed by water, the parallel light exits from an exit surface of the sample cell 3, i.e., the second quartz optical window 10, and enters the optical signal detection system 5 after passing through the converging system 4.
The optical signal detection system 5 is used for splitting and detecting incident light, acquiring light intensity signals of various wavelengths, calculating and processing the light intensity signals to obtain final COD concentration information of the liquid to be detected, and achieving the purpose of rapid and accurate measurement of low-concentration COD in the water body.
In some preferred embodiments, the first plane mirror 7 and the second plane mirror 8 of the sample cell 3 are arranged at an angle θ, which is in the range of 0 to 2 °. When the sample cell 3 is manufactured, the included angle theta between the first plane reflecting mirror 7 and the second plane reflecting mirror 8 is set through the angle measuring device, the measuring optical path is changed, and different included angles theta correspond to different measuring optical paths, so that the measuring range of the COD concentration is changed.
After light enters the sample cell 3, because an included angle theta exists between the first plane reflecting mirror 7 and the second plane reflecting mirror 8, the light is reflected for many times in the sample cell 3, the reflection times of the light in the sample cell 3 determine the measurement optical path, and compared with the traditional linear measurement optical path, the measurement optical path is increased, so that the detection limit of COD concentration is greatly reduced, the detection sensitivity is improved, and the low-concentration detection of COD can be realized.
Therefore, by setting different angles θ between the first plane mirror 7 and the second plane mirror 8 to change the measurement optical length, the COD concentration measurement range can be expanded.
In addition, in the actual test process, the sample cell 3 can be placed on an angle rotating table, the rotating angle of the angle rotating table can be controlled, the angle of the light beam incident on the sample cell 3 can be adjusted slightly (the angle ranges from 0 to 5 degrees), and the reflection times can be changed rapidly, so that the measuring optical path length can be changed.
In some preferred embodiments, the incident light is incident on the first quartz optical window 9 perpendicularly to the sample cell 3, so that the dispersion of the incident light with different wavelengths due to the different refractive indexes of the liquid can be reduced.
In some preferred embodiments, the light source 1 is any one of a xenon lamp broadband light source, a pulsed xenon lamp broadband light source, a deuterium lamp broadband light source, a narrow-band LED, or a laser narrow-band light source.
The function of the collimation system 2 is to obtain parallel light, in some preferred embodiments, the collimation system 2 uses a concave reflector or a quartz collimator; the concave reflector is plated with an ultraviolet enhanced reflecting film; for flexibility of the optical path, it is also possible to adopt a mode in which light is coupled to the optical fiber 6 by a converging mirror and converted into parallel light at the output end of the optical fiber by a collimating mirror.
The converging system 4 has the function of converging parallel light into the detection system, and in some preferred embodiments, the converging system 4 adopts a concave reflector or a quartz converging mirror; the concave reflector is plated with an ultraviolet enhanced reflecting film; for flexibility of the optical path, it is also possible to couple parallel light to the optical fiber 6 by means of a converging mirror, which converges the light at the fiber output end.
In some preferred embodiments, the optical signal detection system 5 is used to perform optical splitting detection on the optical signal, and the optical signal detection system 5 adopts a spectrometer or an optical filter and a detector; the detector is any one of a linear array CCD, an area array CCD, a photodiode array, a photomultiplier tube or a photocell.
In some preferred embodiments, the sample cell 3 is used for holding a water sample to be tested, and the sample cell 3 can be a closed sample cell or an open sample cell; as shown in fig. 4, the closed sample cell is a closed strip hexahedron, and includes a bottom plate and an upper cover plate, and a water inlet 11 and a water outlet 12 are provided at the front and rear ends of the sample cell 3; the left and right surfaces are a first optical reflection end surface and a second optical reflection end surface; the bottom plate and the upper cover plate are made of black opaque materials. As shown in fig. 5, the open sample cell has a rectangular channel for the inflow of the water sample to be measured, and the open sample cell is suitable for being thrown into a water body for online measurement. The open type sample cell is not provided with a bottom plate, an upper cover, a front end face and a rear end face, only comprises a left end face and a right end face, a rectangular channel into which a measured water sample can flow is formed, and the left end face and the right end face are respectively a first optical reflection end face and a second optical reflection end face.
In some preferred embodiments, the reflective optical lens of the device is coated with an ultraviolet-enhanced reflective film to enhance the reflection of light in the ultraviolet band, and the collimating system 2, the first plane mirror 7 and the second plane mirror 8 are coated with an ultraviolet-enhanced reflective film. In order to avoid the damage of the water body to the ultraviolet reflecting film, the first plane reflecting mirror 7 and the second plane reflecting mirror 8 are coated on the surfaces after being selected.
In some preferred embodiments, the lens is a quartz lens to reduce absorption of light in the ultraviolet band and improve transmittance of ultraviolet light, such as: the convergence system 4, the first quartz optical window 9 and the second quartz optical window 10 are quartz lenses. The light source 1 adopts a pulse xenon lamp, and the power is 5 w; the collimating system 2 adopts a concave reflector, the signal acquisition system 5 adopts a fiber spectrometer, and the response wavelength range of the fiber spectrometer is 200-800 nm.
The specific devices and structures in the light source, the collimation system, the convergence system and the optical signal detection system in the above embodiments of the present invention are respectively selected according to application requirements. If any optical lens needing light reflection, light condensation and the like, such as a concave reflector or a plane reflector, is involved in the device, the surface of the lens needs to be plated with an ultraviolet enhancement film to enhance the reflection of ultraviolet band light, and all involved lenses are quartz lenses to improve the ultraviolet transmittance.
Further, the apparatus in the above embodiment of the present invention was tested by configuring COD samples with different concentrations:
COD samples with the concentrations of 0, 0.3, 0.5, 0.8, 1, 1.5, 2 and 4 are prepared respectively, the measurement is performed for 5 times respectively, the light intensity information at 254nm is selected, and the average value is obtained.
The method comprises the steps of putting a COD solution with a prepared concentration into a sample cell 3, enabling light beams emitted by a pulse xenon lamp to be incident on a concave reflector to be changed into parallel light, enabling the parallel light to be vertically incident into the sample cell 3 to be incident into a first quartz light window 9, adjusting an included angle theta between a first plane reflector 7 and a second plane reflector 8 to be a certain appropriate angle, enabling the light beams to be completely emergent from a second quartz light window 10 after being reflected for multiple times in the sample cell 3 and absorbed by water, converging the light beams through a converging lens to be received by a spectrometer to obtain light intensity information of each wavelength, selecting light intensity information at 254nm, measuring the light intensity information for 5 times respectively, taking an average value, and calculating a light absorption value of the concentration at 254 nm.
Sequentially measuring COD samples with the concentrations of 0, 0.3, 0.5, 0.8, 1, 1.5, 2 and 4 for 5 times, selecting light intensity information at 254nm, averaging, and calculating the absorbance value at the concentration of 254nm to obtain the following results:
as shown in Table 1, the results of the measurement of COD solutions of different concentrations at a wavelength of 254nm,
| COD concentration (mg/L) | Absorbance at 254nm |
| 0.3 | 0.0441 |
| 0.5 | 0.0767 |
| 0.8 | 0.1289 |
| 1 | 0.1502 |
| 1.5 | 0.2289 |
| 2 | 0.2965 |
| 4 | 0.5770 |
TABLE 1
Lambert beer's law, i.e. the relationship between the intensity of absorption of a substance at a certain wavelength of light and the concentration of the light-absorbing substance and its liquid layer thickness. As can be seen from the data in table 1 and fig. 6, the absorbance and the COD concentration measured by the apparatus have an ideal linear relationship, and conform to the lambert law.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (8)
1. A low concentration COD measuring device based on spectrum method which characterized in that: the measuring device comprises a light source, a collimation system, a sample cell, a convergence system and an optical signal detection system, wherein the inner wall of the sample cell is provided with a first optical reflection end face and a second optical reflection end face which are opposite, a first quartz optical window and a first plane reflector are sequentially arranged on the first optical reflection end face, and the first quartz optical window is the incident face of the light source; a second plane reflector and a second quartz optical window are sequentially arranged on the second optical reflection end face, and the second quartz optical window is an emergent face of the light source;
the light emitted by the light source is changed into parallel light through the collimation system, the parallel light enters the sample cell through the first quartz light window of the sample cell, the parallel light is emitted from the second quartz light window of the sample cell after being reflected for multiple times by the first plane reflector and the second plane reflector and absorbed by liquid to be detected, and then enters the optical signal detection system after passing through the convergence system; the parallel light is vertically incident to the first quartz light window incidence surface of the sample cell and is used for reducing the dispersion of the light with different wavelengths caused by different liquid refractive indexes during incidence; an included angle is set between the first plane reflecting mirror and the second plane reflecting mirror
By setting the angle of the first plane mirror and the second plane mirror
Changing the measuring optical path, thereby changing the COD concentration measuring range;
the optical signal detection system is used for splitting and detecting incident light, acquiring light intensity signals of various wavelengths, and calculating the light intensity signals to obtain the COD concentration of the detected liquid.
2. A spectroscopy-based low-concentration COD measuring apparatus according to claim 1, wherein: the angle
Take between 0 and 2 deg..
3. A spectroscopy-based low-concentration COD measuring apparatus according to claim 1, wherein: has one or more of the following characteristics:
-the sample cell takes the form of a closed sample cell or an open sample cell;
the closed sample cell is a closed elongated hexahedron comprising a bottom plate and an upper cover plate, and a water inlet and a water outlet are formed in the front end and the rear end of the sample cell;
-said base plate and said upper cover plate are both of black opaque material;
-the open sample cell has a rectangular channel for inflow of the water sample to be measured, the open sample cell being adapted for being plunged into a body of water for on-line measurement.
4. A spectroscopy-based low-concentration COD measuring apparatus according to claim 1, wherein: has one or more of the following technical characteristics:
the rear surfaces of the first and second planar reflectors are coated with ultraviolet-enhanced reflective films to enhance reflection of light in the ultraviolet band;
-said first and second planar mirrors are composed of a stack of quartz glass and uv-enhancing mirrors, respectively.
5. A spectroscopy-based low-concentration COD measuring apparatus according to claim 1, wherein: the light source is any one of a xenon lamp broadband light source, a deuterium lamp broadband light source, a narrow-band LED or a laser narrow-band light source.
6. A spectroscopy-based low-concentration COD measuring apparatus according to claim 1, wherein: has one or more of the following technical characteristics:
-the collimating system employs a concave mirror or a quartz collimating mirror;
-said concave mirror is coated with an ultraviolet enhanced reflective film;
the collimating system is used for improving the flexibility of the optical path in a way that light is coupled to the optical fiber through a converging mirror and changed into parallel light through a collimating mirror at the output end of the optical fiber.
7. A spectroscopy-based low-concentration COD measuring apparatus according to claim 1, wherein: has one or more of the following technical characteristics:
-said converging system uses a concave mirror or a quartz converging mirror;
-said concave mirror is coated with an ultraviolet enhanced reflective film;
the converging system employs parallel light coupling to the optical fiber by means of a converging mirror, and light is converged by the converging mirror at the output end of the optical fiber, for improved flexibility of the optical path.
8. A spectroscopy-based low-concentration COD measuring apparatus according to claim 1, wherein: has one or more of the following characteristics:
-the optical signal detection system employs a spectrometer, or, an optical filter plus a detector;
the detector is any one of a linear array or an area array CCD, a photodiode array, a photomultiplier tube or a photocell.
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